CN110337507A - Cylinder type sputtering target and its manufacturing method - Google Patents
Cylinder type sputtering target and its manufacturing method Download PDFInfo
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- CN110337507A CN110337507A CN201880012802.0A CN201880012802A CN110337507A CN 110337507 A CN110337507 A CN 110337507A CN 201880012802 A CN201880012802 A CN 201880012802A CN 110337507 A CN110337507 A CN 110337507A
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Abstract
The present invention provides a kind of cylinder type sputtering target and its manufacturing method, the manufacturing method of cylinder type sputtering target of the invention includes: base treatment process, and at least one party's coating substrate processing grafting material in the inner peripheral surface on the joint surface as cylinder type target (2) and the outer peripheral surface on the joint surface as cylinder type bushing pipe (3) is to form base treatment layer (11)；And bonding process, after base treatment process, filling with the gap between the bushing pipe (3) that grafting material is filled into cylinder type target (2) and is inserted into the cylinder type target and is solidified, the fusing point or solidus temperature of base treatment grafting material are more than the fusing point or solidus temperature of filling grafting material.
Description
Technical field
The present invention relates to a kind of cylinder type sputtering target being used in sputtering equipment and its manufacturing methods.
This application claims based on April 7th, 2017 in patent application No. 2017-076471 and 2018 3 of Japanese publication
Months 23 days patent application 2018-56467 priority in Japanese publication, and its content is applied at this.
Background technique
It has been known that there is the sputtering equipments sputtered while rotating cylinder type sputtering target.Such as patent document 1 or patent
Shown in document 2, cylinder type sputtering target used in the sputtering equipment is bonded to cylinder type on the outer peripheral surface of cylinder type bushing pipe
The inner peripheral surface of target.
It has been known that there is following joint methods: in the engagement, in the outer peripheral surface and cylinder of the cylinder type bushing pipe for becoming joint surface
On the inner peripheral surface of type target, handled as base treatment by the bonding machine based on ultrasonic welding machine (ultrasonic soldering iron)
It is inserted into cylinder type bushing pipe in cylinder type target, sets therebetween later with the same or similar envelope of grafting material to be formed
The gap for joint portion is set, supplies grafting material in the gap to fill gap.And, it is also known that have as grafting material
And use indium (In).
Patent document 1: Japanese Unexamined Patent Publication 2016-74977 bulletin (A)
Patent document 2: Japanese Unexamined Patent Publication 2014-37619 bulletin (A)
The engagement of cylinder type bushing pipe and cylinder side target needs following series of process: the heating of these bushing pipes and target is based on
The base treatment of base treatment grafting material and its cooling, insertion from bushing pipe to target, therebetween formed between grafting material uses
Gap, assembling, the filling and cooling to gap of reheating, grafting material of target and bushing pipe.
Here, base treatment is following process: target and bushing pipe are added if being illustrated to the base treatment of target and bushing pipe
More than heat to the fusing point of base treatment grafting material, and using ultrasonic soldering iron to the outer peripheral surface of bushing pipe and the inner peripheral surface of target
Coating substrate handles grafting material.
The surface of the base treatment grafting material of target and bushing pipe is by the cooling after base treatment and is used for grafting material
Reheating before the engagement in gap both being filled in and carry out surface oxidation.
By forming the oxidation film of the base treatment bonding material surfaces, the grafting material filled is engaged with base treatment
The contact of material is prevented, and be easy to produce engagement it is bad, be unable to ensure in ultrasonic examination inspection upon engagement set
Bonding area ratio, sometimes the quality of product become it is unqualified.
Become underproof sputtering target about this quality, after to whole heated so that grafting material melts,
It needs to take out target from bushing pipe, is modified the operation of engagement again.On the other hand, with the enlargement for the substrate being sputtered,
Cylinder type target is lengthened out, and is also contemplated that the raising of bond strength.
Summary of the invention
The present invention is to complete in light of this situation, and its object is to prevent because of the grafting material table Jing Guo base treatment
The oxidation film in face and generate that engagement is bad, and the amendment for reducing engagement is operated to improve productivity, and improves target and bushing pipe
Bond strength.
Manufacturing method (hereinafter referred to as " the cylinder type sputtering target of the invention of the cylinder type sputtering target of a mode of the invention
Manufacturing method "), the inner peripheral surface of the outer peripheral surface of cylinder type bushing pipe and cylinder type target is set as joint surface, and by grafting material
It come the gap being filled between joint surface and is engaged, the manufacturing method of the cylinder type sputtering target includes: bases
Science and engineering sequence, in the inner peripheral surface on the joint surface as the cylinder type target and the outer peripheral surface on the joint surface as the cylinder type bushing pipe
In at least one party's coating substrate processing grafting material to form base treatment layer；And bonding process, base treatment process it
Afterwards, by gap of the filling between the bushing pipe that grafting material is filled into the cylinder type target and is inserted into the cylinder type target
In and solidified, the fusing point or solidus temperature of the base treatment grafting material are more than the molten of the filling grafting material
Point or solidus temperature.
In this manufacturing method, the base treatment layer formed in base treatment process is coated in base treatment grafting material
Surface is oxidized in heating in cooling afterwards and when bonding process, and forms oxidation film.In the base treatment grafting material
It, can be by temperature when engaging in the case that fusing point or solidus temperature are higher than the fusing point or liquidus temperature of filling grafting material
Degree is set as the medium temperature of the two.It is set by the temperature, base treatment grafting material is being used for filling grafting material
It is heated in the heating process being filled with solid state shape, therefore oxidation is inhibited, and engages bad reduction.
In the manufacturing method of cylinder type sputtering target of the invention, the base treatment grafting material is that Theil indices are 90 matter
Measure the pure tin or tin alloy of % or more, the filling pure indium or indium alloy that grafting material is that indium content is 85 mass % or more
?.
In this manufacturing method, the junction temperature in bonding process is set as the fusing point (about 157 DEG C) of indium or more and substrate
The fusing point of grafting material is handled hereinafter, thus in the heating in bonding process, the surface of base treatment layer will not melt, therefore
The oxidation of base treatment layer surface caused by being able to suppress because of the heating before engagement.If also, filling grafting material and substrate
Processing grafting material contacts on joint interface, then wetability improves due to the effect of the eutectic reaction of tin and indium, can reduce
It engages bad.Also, as another reason for engaging bad reduction, can enumerate: the oxidation film of base treatment layer surface is tin
Oxide, thus density is smaller compared with filling grafting material, therefore in the gap of cylinder type target and cylinder type bushing pipe
During the filling grafting material for filling molten condition, the oxidation film being stripped from base treatment layer surface is in fusing department
Top floats.According to the effect, after completing splices, oxide is also not easy to remain in filling grafting material.
In this case, the filling is the indium alloy comprising 15 mass % tin below with grafting material.
In the manufacturing method of cylinder type sputtering target of the invention, implement the base treatment process in inert atmosphere
Or at least one of described bonding process.
It can prevent from aoxidizing as much as possible by inert atmosphere, and can be realized further increasing for bond strength.It should
In the case of, in base treatment process, at least since the coating of base treatment grafting material until cooling complete during,
Also, in bonding process, at least since heating to filling grafting material filling complete until during, maintain it is non-live
Property atmosphere.
In the manufacturing method of cylinder type sputtering target of the invention, the bonding process can have reheating operation, should
Reheating operation is by the cylinder type target and the bushing pipe being inserted into the cylinder type target, with the filling grafting material
Fusing point or solidus temperature carry out again more than or lower than the fusing point of the base treatment grafting material or the temperature of solidus temperature
Heating.
About the cylinder type sputtering target (hereinafter referred to as " cylinder type sputtering target of the invention ") of other modes of the invention,
It is inserted into cylinder type bushing pipe in cylinder type target, is formed with packet between the outer peripheral surface of cylinder type bushing pipe and the inner peripheral surface of cylinder type target
It is being incited somebody to action on the section at the joint portion of the central axis relative to the cylinder type bushing pipe at joint portion containing indium and tin
From the joint interface at the joint interface and cylinder type bushing pipe at cylinder type target Yu the joint portion and the joint portion at least
The joint interface of one side to the tin concentration in the range of 10 μ m thicks inside joint portion is set as S1 mass % and by the joint portion
The tin concentration of central portion of thickness direction when being set as S2 mass %, (S1/S2) >=1.5.
In the case where cylinder type target is engaged with cylinder type bushing pipe, before filling grafting material therebetween,
At least one party in the inner peripheral surface of cylinder type target and the outer peripheral surface of cylinder type bushing pipe is pre-coated with as main component with tin
Base treatment material, but as described above, become if generating the concentration gradient of tin in joint portion upon engagement in thickness direction
The state of base treatment layer and joint portion fusion, bond strength improve.In this case, if (S1/S2) less than 1.5, joint portion
Engaging force reduce, it is possible to cylinder type target deviates on cylinder type bushing pipe in sputtering.
In accordance with the invention it is possible to prevent from generating engagement because of the oxidation film of the bonding material surfaces Jing Guo base treatment not
It is good, and the amendment for reducing engagement is operated to improve productivity, and can be improved the bond strength of target and bushing pipe.
Detailed description of the invention
Fig. 1 is the longitudinal section view of the cylinder type sputtering target of embodiments of the present invention.
Fig. 2 is the drawing in side sectional elevation of Fig. 1.
Fig. 3 is the schematic diagram of the component characteristic in the section at the enlarged fragmentary cross section and joint portion indicated in the A of Fig. 1.
Fig. 4 is the flow chart being illustrated to the 1st embodiment of the manufacturing method of cylinder type sputtering target.
Fig. 5 is the longitudinal section view of the state in the manufacturing process in the manufacturing method for indicate the 1st embodiment.
Fig. 6 is the flow chart being illustrated to the 2nd embodiment of the manufacturing method of cylinder type sputtering target.
Fig. 7 A is the longitudinal section view of the state in the manufacturing process in the manufacturing method for indicate the 2nd embodiment.
Fig. 7 B is the longitudinal section view of the state in the manufacturing process in the manufacturing method for indicate the 2nd embodiment.
Specific embodiment
Hereinafter, being carried out with reference to attached drawing to the embodiment of cylinder type sputtering target according to the present invention and its manufacturing method
Explanation.
As shown in Figures 1 and 2, about cylinder type sputtering target 1, cylinder type bushing pipe 3 is inserted into cylinder type target 2, these circles
It is engaged between the inner peripheral surface of cartridge type target 2 and the outer peripheral surface of cylinder type bushing pipe 3 via joint portion 4.In this case, cylinder type
Target 2 and cylinder type bushing pipe 3 are configured with the consistent state of central axis.
There is no particular limitation for the material or size of cylinder type target 2 and cylinder type bushing pipe 3.Such as cylinder type target 2 can make
With the internal diameter being made of the metals such as copper (Cu), silver-colored (Ag), titanium (Ti), silicon (Si), the ceramics such as zinc oxide (AZO) for being doped with aluminium etc.
For the cartridge of 134mm~137mm.Such as cylinder type bushing pipe 3 be able to use by titanium (Ti), stainless steel (SUS) or copper or
Copper alloy constitute outer diameter be 133mm~136mmmm, the cartridge that length is 1m~3m.In this case, cylinder type target 2 with
The outer of cylinder type bushing pipe 3 is configured at via the state that gasket 5 has linked the target 2a for the short size that multiple length are 30cm or so
Week.Gasket 5 after grafting material solidification solidification, is gone in grafting material cooling process at the time of becoming 100 DEG C or more
It removes.In the state of inserting cylinder type bushing pipe 3 in cylinder type target 2,0.5mm~2mm is formed along radial direction therebetween
Gap.In addition, in the gap, be inserted into the spacer 6 for keeping gap as be described hereinafter, with the spacer 6 cylinder together
Type target 2 and cylinder type bushing pipe 3 are integrally formed by joint portion 4.
Joint portion 4 is, for example, the pure indium or indium alloy that indium content is 85 mass % or more, includes 15 mass % tin below.
In this case, cylinder type sputtering target 1 is manufactured after base treatment process by bonding process as be described hereinafter, therefore is being connect
In conjunction portion 4, as shown in figure 3, the concentration gradient of indium (In) and tin (Sn) thickness direction generate, will from cylinder type target 2 with connect
The joint interface and cylinder type bushing pipe 3 in conjunction portion 4 and 10 μ m thick of inside from the joint interface at joint portion 4 to joint portion 4 range
The tin concentration (average value) of interior (the position P1 of Fig. 3) be set as S1 mass % and by the central portion of the thickness direction at joint portion 4 (
When the thickness at joint portion 4 is set as T, from joint interface be T/2 position (the position P2 of Fig. 3)) tin concentration be set as S2 matter
When measuring %, (S1/S2) >=1.5.
Although there is no particular limitation, the upper limit value of the content on the position P2 of indium included in joint portion 4 is
99.99 quality %.Similarly, although there is no particular limitation, the preferred indium content on the position P2 at joint portion 4 is
The 90.00 mass % of mass %~99.97, more preferably 95.00 mass of mass %~99.95 %.
Although there is no particular limitation, the lower limit value of the content on the position P2 of tin included in joint portion 4 is
0.01 mass %.Similarly, although there is no particular limitation, it is preferable that the content of tin included in joint portion 4 is 0.1
The mass % of quality %~5.0, more preferably 0.2 mass of mass %~1.0 %.
Although there is no particular limitation, the upper limit value of S1/S2 is 1500.Similarly, although there is no particular limitation,
It is preferable that the range of S1/S2 is 5≤(S1/S2) <, 1000, further preferably 20≤(S1/S2) < 100.
The manufacturing method > of < cylinder type sputtering target
Then, the manufacturing method about cylinder type sputtering target 1 is illustrated its 1st embodiment.Implement the 1st
In mode, as illustrated in the flow diagram of fig. 4, successively implement: the heating process of cylinder type bushing pipe 3 and cylinder type target 2；Based on bases
Manage the base treatment process of grafting material；Base treatment grafting material cooling process；Cylinder type bushing pipe 3 is inserted to cylinder type target 2
Enter and form therebetween the assembling procedure assembled in the state of grafting material gap；Cylinder type target 2 and circle
The reheating operation of cartridge type bushing pipe 3；Grafting material filling work procedure filling being filled in grafting material in gap；And engagement material
Expect cooling process.Hereinafter, being illustrated to process sequence.
(heating process)
Cylinder type target 2 and cylinder type bushing pipe 3 are heated, and will be become in their the cylinder type target 2 on joint surface
The outer peripheral surface of circumferential surface and cylinder type bushing pipe 3 is heated to the temperature of the fusing point (or liquidus temperature) of base treatment grafting material or more
Degree.Such as in the case where using pure tin (purity: 99.8 mass % or more) as base treatment grafting material, it is heated to be
232 DEG C or more.
(base treatment process)
In heating process, on the inner peripheral surface for the cylinder type target 2 for being set as heated condition and the outer peripheral surface of cylinder type bushing pipe 3
The base treatment grafting material of molten condition is coated respectively.In this case, on one side with the ultrasonic soldering iron for carrying heater
(illustration omitted) applies ultrasonic activation, coats base treatment grafting material on one side, thus the inner peripheral surface and circle of cylinder type target 2
The removal etc. of dirt or oxidation film on the outer peripheral surface of cartridge type bushing pipe 3 is promoted, and can make base treatment grafting material and this
A little surface fusions.As base treatment grafting material, pure tin or Theil indices can be used as the tin alloy of 90 mass % or more.
As tin alloy, the preferably indium stannum alloy containing 15 mass % indiums below.Indium additive amount is more than 15 mass %
The fusing point (liquidus temperature) of tin alloy become 180 DEG C hereinafter, when engagement carries out the oxidations of engagement surface by heating, have
Bond strength reduction in possible oxide entrapment joint portion.
Although there is no particular limitation, the upper limit value of the Theil indices of base treatment grafting material is 100 mass %.Together
Sample, although there is no particular limitation, it is preferable that the Theil indices of base treatment grafting material are 90 matter of mass %~100
Measure %, more preferably 95 mass of mass %~100 %.
As base treatment grafting material, in addition to this, additionally it is possible to using containing 0.7 mass % copper below (such as Sn-
The alloy of 0.7Cu) copper-tin alloy, the red brass containing 9 mass % zinc below, contain 3.5 mass % it is below silver
Silver-tin alloy etc..
If implementing the base treatment process in the inert atmospheres such as argon gas, nitrogen, it is able to suppress and passes through base treatment
Grafting material and the oxidation on the surface of base treatment layer formed.The inert atmosphere is at least since the coating of base treatment material
To the base treatment grafting material in next base treatment grafting material cooling process it is cooling complete until during into
Row maintains.
(base treatment grafting material cooling process)
The cylinder type target 2 for being coated with base treatment grafting material and cylinder type bushing pipe 3 are cooled to room temperature (20 DEG C), thus
Cured substrate handles grafting material.Become as a result, and is formd on the inner peripheral surface of cylinder type target 2 and the outer peripheral surface of cylinder type bushing pipe
The state of base treatment layer 11.As the thickness of the base treatment layer 11, there is no particular limitation, it is preferred that being 10 μm or more
And 200 μm or less.In the case where the thickness of base treatment layer 11 is less than 10 μm, it is difficult to make base treatment grafting material and cylinder
Type target 2 and cylinder type bushing pipe 3 fully fuse, also, the materials statement face of cylinder type target 2 and cylinder type bushing pipe 3 is easily exposed,
Later, it is bad that engagement is easy to produce when being filled with filling grafting material.If the thickness of base treatment layer 11 is more than 200 μm,
Then grafting material accumulates in lower section because of gravity after the substrate treatment, and when assembling can not make cylinder type bushing pipe 3 pass through cylinder type
Target 2, manufacture becomes difficult sometimes.
Although there is no particular limitation, preferred base treatment layer 11 with a thickness of 30 μm~150 μm, it is further excellent
It is selected as 50 μm~100 μm.
In addition, in the base treatment grafting material cooling process, after can also mechanically removing solidification at room temperature
The oxide on 11 surface of base treatment layer.It is reached below oxide alternatively, being formed to the oxide on 11 surface of base treatment layer
Scratch until grafting material.In this way, removing the oxide on all or part of 11 surface of base treatment layer at room temperature, thus
The fusion of base treatment grafting material and filling grafting material is further improved in grafting material filling work procedure.
(assembling procedure)
As shown in figure 5, firstly, have can configure cylinder type bushing pipe 3 end recess portion 13a fixed station 13 on,
Cylinder type target 2 is loaded in a manner of surrounding recess portion 13a.Then, cylinder type bushing pipe 3 is inserted into cylinder type target 2, at them
Between the state of circumferentially spaced constant clearance be configured on coaxial.In order to be set as constant clearance in the circumferential, in cylinder type target 2
The configuration space object 6 between cylinder type bushing pipe 3.As the spacer 6, the line being preferably made of metals such as copper or stainless steels
Material uses the wire rod of the corresponding outer diameter in gap between cylinder type target 2 and cylinder type bushing pipe 3.Circumferential direction along gap is between grade
Every being inserted into more such as three spacers 6, cylinder type target 2 and cylinder type are thus circumferentially configured on the same axis with constant clearance
Bushing pipe 3.
(reheating operation)
The cylinder type target 2 and cylinder type bushing pipe 3 assembled as previously described is heated by heater (illustration omitted), is set as
The filling fusing point (or solidus temperature) of the fusing point (or liquidus temperature) of grafting material or more and base treatment grafting material
Temperature below.In this way, passing through fusing point that cylinder type target 2 and cylinder type bushing pipe 3 are heated to be to filling grafting material (or liquid phase
Line temperature) more than and base treatment grafting material fusing point (or solidus temperature) temperature below, base treatment layer 11 will not
Melting, and it is able to suppress oxidation caused by heating.
Although there is no particular limitation, it is preferable that the temperature of the process of reheating is 145 DEG C more than or lower than 200 DEG C,
More preferably 160 DEG C more than or lower than 180 DEG C.
Similarly, the heating time for preferably reheating process is 10 minutes~3 hours, and more preferably 30 minutes~2 is small
When.
(grafting material filling work procedure)
The cylinder type target 2 and cylinder type bushing pipe 3 for configuring heated condition along the vertical direction, enclose therebetween by gasket 5
In the state of the lower end of gap, the filling engagement material of filling molten condition is such as indicated with the arrow B of Fig. 5 from the top in gap
Material.Filling is trapped in by spacer 6 lower part in the gap kept with grafting material, and is increasingly towards top and is filled.?
The upper end of gap is provided with the pallet 12 of the filling grafting material for receiving to overflow from gap, and filling is filled with grafting material
In the pallet 12 until overflowing.
As the filling grafting material, the preferably indium alloy containing 15 mass % tin below.As filling with connecing
The tin concentration of condensation material is more than the indium alloy of 15 mass %, and when tin concentration is more than 15 mass % and 79 mass % or less, fusing point drops
Low is to soften in sputtering because the conduction from cylinder type target 2 is hot, it is possible to which cylinder type target 2 is served as a contrast in cylinder type lower than 140 DEG C
It moves and deviates on pipe 3.Also, if 79 mass % or more, then according to the temperature difference of solidus and liquidus curve, when filling is with connecing
Condensation material solidify when, be easy to produce with shrinkage cavity (Yin Testis) engagement it is bad.
If the filling is filled in the gap between cylinder type target 2 and cylinder type bushing pipe 3 with grafting material, such as preceding institute
It states, since the main component of base treatment layer 11 is tin, the main component of filling grafting material is indium, therefore these tin and indium
It is improved by the effect wetability of eutectic reaction.Also, since the oxide of base treatment layer surface is the oxide of tin, because
This density compared with filling grafting material is smaller, by overflowing grafting material in the top in gap, can make oxide
Float and is removed from gap.Therefore, residual oxide is not easy in joint portion.
As filling grafting material, aforementioned indium alloy can not only be applied, and as with base treatment grafting material
Combination and can apply table 1 grafting material.
[table 1]
| Base treatment grafting material | Grafting material is used in filling | |
| 1 | Pure Sn (99.99 mass % of purity or more) | Pure In (99.9 mass % of purity or more) |
| 2 | The mass of In:0~15 %, remainder: Sn | The mass of Sn:0~15 %, remainder: In |
| 3 | Cu:0.7 mass % or less, remainder: Sn | Pure In (99.9 mass % of purity or more) |
| 4 | The mass of Zn:0~9 % or less, remainder: Sn | Pure In (99.9 mass % of purity or more) |
| 5 | The mass of Ag:0~3.5 % or less, remainder: Sn | Pure In (99.9 mass % of purity or more) |
By being set as combination shown in table 1, the fusing point of base treatment grafting material is set as than filling grafting material
Fusing point is high, can set junction temperature in the intermediate region of the two, reduces with undesirable amendment operation is engaged, in turn, can
Improve bond strength.
Also, about the density of grafting material and oxide, as shown in table 2.
[table 2]
| Grafting material | Density (g/cm3) |
| In (wherein, in the fluid density of fusing point) | 7.02 |
| Sn (wherein, in the fluid density of fusing point) | 6.99 |
| Indium oxide (In2O3) | 7.18 |
| Tin oxide (SnO2) | 6.85 |
As shown in table 2, tin (Sn) is used as base treatment grafting material, uses indium as filling grafting material
(In), the density of the density ratio indium of the oxidation film (tin oxide) thus formed on the surface of base treatment layer is small.To, by
The filling grafting material being made of indium is filled in the gap of cylinder type target 2 and cylinder type bushing pipe 3, can make base treatment layer table
The tin oxide in face floats and removes.
In addition, by implementing reheating operation under inert atmosphere, grafting material filling work procedure (is completed at least to filling
Until during), be able to suppress the oxidation of grafting material, and further increase bond strength.
(grafting material cooling process)
After being filled with filling grafting material in the gap of cylinder type target 2 and cylinder type bushing pipe 3, be cooled into
Row solidification, removes unwanted attachment etc. and removes, and thus completes cylinder type target 2 and cylinder type bushing pipe 3 passes through joint portion 4
The cylinder type sputtering target 1 being integrally formed.
The cylinder type sputtering target 1 is after tin is formd base treatment layer 11 as main component, by with indium
The sputtering target making filling grafting material as main component and being integrally formed, therefore as previously mentioned, in its thickness in joint portion 4
Spend the concentration gradient that direction generates tin and indium.Also, the residual of the oxide on 11 surface of base treatment layer is inhibited, therefore base
Bottom process layer 11 is fused with joint portion 4 and is integrally formed, and it is bad can to reduce engagement, and improve bond strength.
In this case, will be from the joint interface at cylinder type target 2 Yu joint portion 4 and cylinder type bushing pipe 3 and joint portion 4
Tin concentration of the joint interface into the thickness range of 10 μm of the inside at joint portion 4 is set as S1 mass %, by the thickness side at joint portion
To the tin concentration of central portion be set as S2 mass % when, (S1/S2) >=1.5.(if S1/S2) < 1.5, the engagement at joint portion 4
Power reduces, it is possible to which cylinder type target 2 deviates on cylinder type bushing pipe 3 in sputtering.
In addition, in the foregoing embodiment, after being assembled in cylinder type target 2 and cylinder type bushing pipe 3 on coaxial, from it
The top in gap has supplied molten filling grafting material, but can also by with method phase documented by patent document 2
With method be filled.
The flow chart of the situation is shown in Figure 6.From (heating process) to (base treatment grafting material cooling process), and it is preceding
The case where stating the manufacturing method of the 1st embodiment is identical.Later, instead of load cylinder type target 2 fixed station 13 and use has
The fixture for storing the recess portion of the filling grafting material of molten condition, on the fixture 14, to be configured at the surface of recess portion 15
Mode via the vertically supporting cylinder type target 2 of gasket 5.Also, grafting material is heated in the recess portion of fixture 14 15, with preparatory
Molten condition stores (grafting material melting process).Moreover, as shown in Figure 7 A, lower end will be set as by interim sealing bolt 16
The cylinder type bushing pipe 3 of closed state is inserted into cylinder type target 2, and passes through 2 He of heater (illustration omitted) Lai Jiare cylinder type target
Cylinder type bushing pipe 3 is set as the fusing point (or liquidus temperature) of filling grafting material or more and base treatment grafting material
Fusing point (or solidus temperature) temperature below (reheating operation).Then, between the cylinder type bushing pipe 3 and cylinder type target 2
Gap in, from below gradually fill molten condition filling grafting material F.As shown in Figure 7 B, if filling grafting material F
It spills into the pallet 12 of the upper end of cylinder type target 2, then fills completion (grafting material filling work procedure).In this embodiment,
Grafting material filling work procedure is also the process for assembling cylinder type target 2 and cylinder type bushing pipe 3.
In addition, in the foregoing embodiment, being applied in the inner peripheral surface of cylinder type target 2 and the outer peripheral surface both sides of cylinder type bushing pipe 3
Cloth base treatment grafting material, if but any surface be in the state being easily wetted with grafting material with filling, about this
Surface can be omitted the coating of base treatment grafting material.
Embodiment
1 > of < embodiment
Prepared the silicon (Si) for being doped with boron (B) cylinder type target (0.05 Ω cm of resistivity, internal diameter: 137mm, outer diameter:
157mm, length: 200mm, hereinafter referred to as Si-TG) 10, pure titanium (Ti) rounding cartridge type bushing pipe (internal diameter: 125mm, outer diameter:
135mm, length: 600mm, hereinafter referred to as Ti-BT) 5 pieces.
The outer peripheral surface of Si-TG is heated using mantle heater, until the inner peripheral surface temperature of Si-TG reaches 240
Until~260 DEG C.250 DEG C or so are kept the temperature at, and pure tin (Sn) is used as base treatment grafting material, in air atmosphere
In base treatment is carried out to the inner peripheral surface of Si-TG by ultrasonic soldering iron after, be cooled to room temperature.
The outer peripheral surface temperature for recycling hot wind on the inner peripheral surface of Ti-BT, and being heated to Ti-BT reaches 240~260 DEG C
Only.250 DEG C or so are kept the temperature at, and pure tin (Sn) is used as base treatment grafting material, by super in air atmosphere
Sound wave soldering iron carries out base treatment to the outer peripheral surface of Ti-BT, and is cooled to room temperature.
After the substrate treatment, each 2 Si-TG are configured to the set position of Ti-BT.It is clamped between cylinder type target
Heat resistance fluororesin gasket (thickness is about 0.6mm), in case grafting material leaks in filling grafting material.In addition, closing
In the assembling of Ti-BT and Si-TG, diameter: 0.6mm copper wire rod (spacer) is carried out with about 120 ° 3 positions that are spaced in
Insertion, forms grafting material filling gap between Si-TG and Ti-BT.
The filling of grafting material after being formed about gap heats Si- by mantle heater in an atmosphere
The outer peripheral surface of TG passes through Japanese Unexamined Patent Publication 2014-37619 after the inner peripheral surface temperature of Ti-BT is maintained at 180 DEG C or so
Shown in method (Fig. 6, Fig. 7 A and Fig. 7 B shown in method), pure indium (In) is carried out as grafting material from lower part towards top
Filling.In topmost, grafting material is overflowed, and floats oxide.It is total that No.1~5 are produced using identical process
5 cylinder type sputtering targets.
After cooling, bonding area ratio is measured by ultrasonic examination check device.Bonding area ratio is to exclude
Ratio of the area relative to the gross area on the joint surface of Si-TG and Ti-BT is completed in the engagement of engagement bad position.On joint surface
Product ratio is evaluated as qualification in the case where being 95% or more.In this case, in the case where not becoming qualified by once engaging,
Grafting material is melted and removed and then it is secondary be re-engaged, and measure bonding area ratio.
Also, by the sample of No.1, radially acquire 20 from arbitrary position and include diameter: the joint portion of 20mm is connect
Strength detection sample is closed, and is provided in tension test.The average value of 20 intensity is set as to the tensile strength at joint portion.
Also, by the sample of No.1 make section structure observation sample, and with 2000 times of multiplying power to joint interface into
Observation is gone.Respectively in the range of about 10 μm (the P1 point of Fig. 3) from the joint interface of the joint interface of Ti-BT and Si-TG, lead to
It crosses EPMA and quantitative analysis is implemented to tin (Sn) concentration with about 1 μm of beam diameter.In this case, by the joint interface of Ti-BT
Side is set as the side BT interface, and the joint interface side of Si-TG is set as the interface TG, and the tin concentration of the P1 point near the interface of the side BT is set as
The tin concentration of P1 point near the interface of the side TG is set as ST, and their average value (ST+SB)/2 is set as S1 by SB.Moreover,
In identical sample, by EPMA to the central part of filling grafting material (from the position of each joint interface about 0.5mm: Fig. 3's
P2 point) tin (Sn) concentration (S2) carry out quantitative analysis, and found out S1/S2.
2 > of < embodiment
As base treatment grafting material, Sn-1 weight %In (224 DEG C of No.6, fusing point), Sn-5 weight %In are used
(215 DEG C of No.7, fusing point), Sn-10 weight %In (200 DEG C of No.8, fusing point), by base treatment temperature be set to 240 DEG C,
230 DEG C and 215 DEG C, in addition to this, cylinder type sputtering target is manufactured in the same manner as in Example 1, after cooling, by ultrasound
Wave inspection check device measures bonding area ratio.Also, after ultrasonic examination inspection terminates, similarly to Example 1
Ground makes bond strength measurement sample and section observation sample, and implements tension test and the tin (Sn) based on EPMA
The quantitative analysis of concentration.
3 > of < embodiment
As base treatment grafting material, Sn-3.5 weight %Ag (221 DEG C of No.9, fusing point), Sn-9 weight %Zn are used
(198 DEG C of No.10, fusing point), Sn-0.7 weight %Cu (227 DEG C of No.11, fusing point), is set to 240 for base treatment temperature
DEG C, 215 DEG C and 240 DEG C, in addition to this, in the same manner as in Example 1 manufacture cylinder type sputtering target, after cooling, by
Ultrasonic examination check device measures bonding area ratio.Also, after ultrasonic examination inspection terminates, with embodiment 1
Similarly, bond strength measurement sample and section observation sample are made, and implements tension test and the tin based on EPMA
(Sn) quantitative analysis of concentration.
4 > of < embodiment
As filling grafting material, In-5 weight %Sn, (150 DEG C of No.12, fusing point), In-10 weight %Sn are used
(144 DEG C of No.13, fusing point), In-15 weight %Sn (140 DEG C of No.14, fusing point), is set to 165 DEG C, 160 for junction temperature
DEG C and 155 DEG C, in addition to this, in the same manner as in Example 1 manufacture cylinder type target, after cooling, by ultrasonic examination
Check device measures bonding area ratio.Also, after ultrasonic examination inspection terminates, similarly to Example 1, production
Bond strength measurement sample and section observation sample, and implement determining for tension test and tin (Sn) concentration based on EPMA
Amount analysis.
5 > of < embodiment
Other than base treatment process and/or bonding process are set as nitrogen atmosphere, make in the same manner as in Example 1
Produce 3 cylinder type sputtering targets (No.15~17).
After cooling, bonding area ratio is measured by ultrasonic examination check device.
Also, by the sample of No.15, bond strength measurement sample is made similarly to Example 1 and section observation is used
Sample, and implement the quantitative analysis of tension test and tin (Sn) concentration based on EPMA.
< conventional example >
The outer peripheral surface temperature of Si-TG is maintained at 180 by the outer peripheral surface that Si-TG is heated using mantle heater
DEG C or so temperature, and by pure indium (In) be used as base treatment grafting material, in an atmosphere by ultrasonic soldering iron to Si-
The inner peripheral surface of TG has carried out base treatment.
It recycles hot wind on the inner peripheral surface of Ti-BT, the outer peripheral surface temperature of Ti-BT is also maintained to 180 DEG C or so of temperature
Degree, and pure indium (In) is used as base treatment grafting material, base has been carried out by outer peripheral surface of the ultrasonic soldering iron to Ti-BT
Bottom reason.
After the substrate treatment, Si-TG each 1 is inserted into the set position of Ti-BT.It is clamped between cylinder type target
Heat resistance fluororesin gasket (about 0.6mm), in case grafting material leaks in the bonding.In addition, about Ti-BT and Si-TG
Assembling, by diameter: 0.6mm copper wire rod (spacer)) be inserted into about 120 ° 3 positions that are spaced in, Si-TG with
Grafting material filling gap is formd between Ti-BT.
The periphery of Si-TG is heated in the filling of grafting material after being formed about gap by mantle heater
Face passes through side shown in Japanese Unexamined Patent Publication 2014-37619 after the inner peripheral surface temperature of Ti-BT is maintained at 180 DEG C or so
Method (Fig. 6, Fig. 7 A and Fig. 7 B shown in method) is filled with pure indium (In) as grafting material from lower part towards top.Most upper
Grafting material is overflowed in portion, and floats oxide.Using identical process, produce 5 cylinder type targets (No.18~
No.22)。
After cooling, bonding area ratio is measured by ultrasonic examination check device.
Also, by the sample of No.18, making 20 from arbitrary position includes diameter: the engagement at the joint portion of 20mm is strong
Test sample is spent, and is provided in tension test.
< comparative example >
Si-TG, Ti-BT use Sn-20 weight %In (136 DEG C of No.23, fusing point), Sn-30 weight %In (No.24,
125 DEG C of fusing point) be used as base treatment grafting material, and base treatment temperature is set to 160 DEG C and 135 DEG C, except this with
Outside, manufacture cylinder type target is measured by ultrasonic examination check device and is connect after cooling in the same manner as in Example 1
Close area ratio.Also, after ultrasonic examination inspection terminates, similarly to Example 1, production bond strength measurement examination
Sample and section observation sample, and implement the quantitative analysis of tension test and tin (Sn) concentration based on EPMA.
Manufacturing condition and rate of engagement about each sample are shown in table 3, the knot analyzed about tensile strength and tin concentration
Fruit is shown in table 4.In table 3, rate of engagement is set as qualified for 95% or more.
In addition, in table 3, the fusing point for the case where base treatment grafting material is alloy indicates solidus temperature or eutectic
The fusing point for the case where point, filling with grafting material are alloy indicates liquidus temperature.In table 3 in documented manufacturing condition,
About the atmosphere of base treatment process and the atmosphere of filling work procedure, used atmosphere is indicated by " √ ", and by meaning not
Applicable " N/A " (Not Applicable) indicates the atmosphere of non-use.
[table 3]
[table 4]
As shown in Table 3, by using filling grafting material more low-melting than base treatment grafting material, engagement
Rate (area ratio) is higher for 95% or more.In the prior embodiment, also available 95% or more rate of engagement, but it is 2 times
It is above to correct engaging as a result, qualified rate of engagement and once engaging as 95% or more is 80%.In contrast,
In embodiment, 95% or more rate of engagement can be obtained in all samples by once engaging, it is known that compared with conventional example
Productivity is excellent.Wherein, it is implemented under inert atmosphere in base treatment process or the embodiment of grafting material filling work procedure,
Rate of engagement is especially high.
Also, as shown in table 4, if the Theil indices of base treatment grafting material are 90 mass % or more, filling engagement material
The indium content of material is 85 mass % or more, then the tin concentration distribution (S1/S2) at joint portion becomes 1.5 or more, can get high connect
Close intensity.
Industrial availability
The present invention can effectively produce the cylinder type sputtering target of high-quality.
Symbol description
1- cylinder type sputtering target, 2- cylinder type target, 2a- target, 3- cylinder type bushing pipe, the joint portion 4-, 5- gasket, the interval 6-
Object, 11- base treatment layer, 12- pallet, 13- fixed station, 14- fixture, 15- recess portion, the interim sealing bolt of 16-.
Claims (5)
1. a kind of manufacturing method of cylinder type sputtering target, the inner peripheral surface of the outer peripheral surface of cylinder type bushing pipe and cylinder type target is set as
Joint surface, and be filled with the gap between joint surface by grafting material and engaged, the cylinder type sputtering target
Manufacturing method is characterised by comprising:
Base treatment process, the inner peripheral surface on the joint surface as the cylinder type target and the engagement as the cylinder type bushing pipe
At least one party's coating substrate processing grafting material in the outer peripheral surface in face is to form base treatment layer；And
Filling is filled into the cylinder type target with grafting material and is inserted into this by bonding process after base treatment process
In the gap between the bushing pipe in cylinder type target and solidified,
The fusing point or solidus temperature of the base treatment grafting material are more than the fusing point or solid phase that grafting material is used in the filling
Line temperature.
2. the manufacturing method of cylinder type sputtering target according to claim 1, which is characterized in that
The base treatment grafting material is the pure tin or tin alloy that Theil indices are 90 mass % or more, filling engagement material
Material is the pure indium or indium alloy that indium content is 85 mass % or more.
3. the manufacturing method of cylinder type sputtering target according to claim 1 or 2, which is characterized in that
Implement at least one of the base treatment process or described bonding process in inert atmosphere.
4. the manufacturing method of cylinder type sputtering target according to any one of claim 1 to 3, which is characterized in that
The bonding process has:
Reheating operation, by the cylinder type target and the bushing pipe being inserted into the cylinder type target, with filling engagement
The fusing point or solidus temperature of material are more than or lower than the fusing point of the base treatment grafting material or the temperature of solidus temperature
It is reheated.
5. a kind of cylinder type sputtering target, which is characterized in that
It is inserted into cylinder type bushing pipe in cylinder type target, is formed between the outer peripheral surface of cylinder type bushing pipe and the inner peripheral surface of cylinder type target
There is the joint portion comprising indium and tin, on the section at the joint portion of the central axis relative to the cylinder type bushing pipe,
By from the joint interface of the joint interface at cylinder type target and the joint portion and cylinder type bushing pipe and the joint portion to
The joint interface of a few side to the tin concentration in the range of 10 μ m thicks inside joint portion is set as S1 mass % and by the engagement
When the tin concentration of the central portion of the thickness direction in portion is set as S2 mass %, S1/S2 >=1.5.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017-076471 | 2017-04-07 | ||
| JP2017076471 | 2017-04-07 | ||
| JP2018-056467 | 2018-03-23 | ||
| JP2018056467A JP2018178251A (en) | 2017-04-07 | 2018-03-23 | Cylindrical sputtering target and manufacturing method of the same |
| PCT/JP2018/014240 WO2018186385A1 (en) | 2017-04-07 | 2018-04-03 | Cylindrical sputtering target, and production method therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110337507A true CN110337507A (en) | 2019-10-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201880012802.0A Pending CN110337507A (en) | 2017-04-07 | 2018-04-03 | Cylinder type sputtering target and its manufacturing method |
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| JP (1) | JP2018178251A (en) |
| CN (1) | CN110337507A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111468799A (en) * | 2020-04-22 | 2020-07-31 | 宁波江丰电子材料股份有限公司 | Welding method of ceramic rotary target |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7172580B2 (en) * | 2018-12-26 | 2022-11-16 | 三菱マテリアル株式会社 | Manufacturing method of cylindrical sputtering target |
| JP7120111B2 (en) * | 2019-03-25 | 2022-08-17 | 三菱マテリアル株式会社 | Manufacturing method of cylindrical sputtering target |
| CN110408897B (en) * | 2019-08-13 | 2023-05-05 | 北京航大微纳科技有限公司 | Vertical binding device and binding method for rotary target |
| JP2021055120A (en) * | 2019-09-27 | 2021-04-08 | 三菱マテリアル株式会社 | Cylindrical sputtering target and method for manufacturing the same |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61291967A (en) * | 1985-06-18 | 1986-12-22 | Matsushita Electric Ind Co Ltd | Target for sputtering |
| CN1363716A (en) * | 2000-12-19 | 2002-08-14 | W.C.贺利氏股份有限两合公司 | Manufacture of tubular targets |
| CN101490290A (en) * | 2006-07-17 | 2009-07-22 | 豪梅公司 | Method of making sputtering target and target produced |
| JP2012132065A (en) * | 2010-12-21 | 2012-07-12 | Tosoh Corp | Cylindrical sputtering target and method for manufacturing the same |
| CN103620082A (en) * | 2011-04-29 | 2014-03-05 | 普莱克斯S.T.技术有限公司 | Method of forming a cylindrical sputter target assembly |
| CN104066700A (en) * | 2012-01-18 | 2014-09-24 | 三井金属矿业株式会社 | Ceramic cylindrical sputtering target and method for producing same |
| CN104532200A (en) * | 2014-12-24 | 2015-04-22 | 四川亚力超膜科技有限公司 | Columnar rotation magnetic control sputtering target |
| CN104818459A (en) * | 2014-02-04 | 2015-08-05 | Jx日矿日石金属株式会社 | Sputtering target and manufacturing method therefor |
| CN104919080A (en) * | 2013-07-08 | 2015-09-16 | Jx日矿日石金属株式会社 | Sputtering target and method for manufacturing same |
| CN105308002A (en) * | 2014-02-18 | 2016-02-03 | 三井金属矿业株式会社 | Ito sputtering target material and method for producing same |
| JP2016023325A (en) * | 2014-07-17 | 2016-02-08 | 住友金属鉱山株式会社 | Joining material sheet and method for manufacturing cylindrical sputtering target |
| CN106460162A (en) * | 2014-05-21 | 2017-02-22 | 贺利氏德国有限责任两合公司 | Cusn, cuzn and cu2znsn sputter targets |
-
2018
- 2018-03-23 JP JP2018056467A patent/JP2018178251A/en not_active Withdrawn
- 2018-04-03 CN CN201880012802.0A patent/CN110337507A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61291967A (en) * | 1985-06-18 | 1986-12-22 | Matsushita Electric Ind Co Ltd | Target for sputtering |
| CN1363716A (en) * | 2000-12-19 | 2002-08-14 | W.C.贺利氏股份有限两合公司 | Manufacture of tubular targets |
| CN101490290A (en) * | 2006-07-17 | 2009-07-22 | 豪梅公司 | Method of making sputtering target and target produced |
| JP2012132065A (en) * | 2010-12-21 | 2012-07-12 | Tosoh Corp | Cylindrical sputtering target and method for manufacturing the same |
| CN103620082A (en) * | 2011-04-29 | 2014-03-05 | 普莱克斯S.T.技术有限公司 | Method of forming a cylindrical sputter target assembly |
| US20140124365A1 (en) * | 2011-04-29 | 2014-05-08 | Dieter Wurczinger | Method of forming a cylindrical sputter target assembly |
| CN104066700A (en) * | 2012-01-18 | 2014-09-24 | 三井金属矿业株式会社 | Ceramic cylindrical sputtering target and method for producing same |
| CN104919080A (en) * | 2013-07-08 | 2015-09-16 | Jx日矿日石金属株式会社 | Sputtering target and method for manufacturing same |
| CN104818459A (en) * | 2014-02-04 | 2015-08-05 | Jx日矿日石金属株式会社 | Sputtering target and manufacturing method therefor |
| CN105308002A (en) * | 2014-02-18 | 2016-02-03 | 三井金属矿业株式会社 | Ito sputtering target material and method for producing same |
| CN106460162A (en) * | 2014-05-21 | 2017-02-22 | 贺利氏德国有限责任两合公司 | Cusn, cuzn and cu2znsn sputter targets |
| JP2016023325A (en) * | 2014-07-17 | 2016-02-08 | 住友金属鉱山株式会社 | Joining material sheet and method for manufacturing cylindrical sputtering target |
| CN104532200A (en) * | 2014-12-24 | 2015-04-22 | 四川亚力超膜科技有限公司 | Columnar rotation magnetic control sputtering target |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111468799A (en) * | 2020-04-22 | 2020-07-31 | 宁波江丰电子材料股份有限公司 | Welding method of ceramic rotary target |
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|---|---|
| JP2018178251A (en) | 2018-11-15 |
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